CN110927189B - Method for EBSD (electron back scattering diffraction) rapid characterization of texture - Google Patents
Method for EBSD (electron back scattering diffraction) rapid characterization of texture Download PDFInfo
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- CN110927189B CN110927189B CN201911260147.3A CN201911260147A CN110927189B CN 110927189 B CN110927189 B CN 110927189B CN 201911260147 A CN201911260147 A CN 201911260147A CN 110927189 B CN110927189 B CN 110927189B
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- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
Abstract
The invention relates to a method for rapidly characterizing a texture by EBSD (electron microscopic imaging), in particular to the technical field of electron microscopic imaging. The method specifically comprises the following steps: s1: obtaining a sample and obtaining the overall size of the sample; s2: obtaining a crystal grain topography of the sample; s3: digitizing the crystal grain topography and recording the position coordinates of the central point of each crystal grain; s4: calibrating the center point of each crystal grain to obtain the crystal orientation of the center of each crystal grain; s5: generating EBSD data of the calibrated area; s6: and obtaining the texture information of the sample according to the EBSD data of the calibration area. The technical problem of how to improve the EBSD characterization efficiency and accuracy of the texture of the crystalline material is solved, and the method is suitable for obtaining large-area crystallographic orientation information of the crystalline material and calculating the accurate macro texture of the material.
Description
Technical Field
The invention relates to the technical field of electron microscopic imaging, in particular to a method for quickly characterizing a texture by EBSD.
Background
Since the invention of the 20 th 90 s, the Electron Back Scattering Diffraction (EBSD) technology has been developed in the field of microstructure characterization (such as phase identification and phase distribution, grain boundary characteristics, grain morphology, micro-domain texture analysis, etc.), and is now widely used. In EBSD, the surface of the sample makes an angle of 70 ° with the electron beam, and when the electron beam strikes the surface of the sample, the generated backscattered electrons are diffracted on the surface of the sample to form a Ki kuch i pattern, which contains the crystallographic information (crystal phase composition and crystallographic orientation information) of the spot, and the pattern is recorded by a high-speed CCD camera, and the phase composition and the crystallographic orientation of the spot can be characterized by computer processing. After completing the calibration of one point, the computer automatically controls the electron beam to move to the next point by the set step length for calibration. This step size is typically 1/10 to 1/5 of the grain size on the sample. The smaller the step size, the finer the final reconstructed image, and the more accurate the calculated texture.
However, the smaller the step size, the more points need to be marked to characterize the same area of the sample surface, which means that it becomes very difficult to accurately characterize the crystallographic features of a large area of the sample surface. A high quality EBSD-oriented reconstruction often requires several, even tens of hours of calibration, which takes up a large number of equipment. Usually, the number of calibration points per EBSD map does not exceed 500 × 500 to 250000, and the number of covered grains is about 2000 to 10000, which is much smaller than the number of grain sizes counted by the conventional XD method. And severe difficulties are encountered in calibrating the following two types of samples:
1. coarse crystals and fine crystals (mixed crystals). At this time, the step length can only be set according to the size of fine crystal grains, otherwise, many crystal grains will be missed, and the marked area is difficult to be large.
2. Coarse grained samples. Some samples with grain size of hundreds of microns cannot cover a large area due to the limitation of the field of view of the scanning electron microscope, and the optical system of the scanning electron microscope has the problem of distortion at low power, and when the edge area is calibrated at low power, the electron beam is obliquely incident on the surface of the sample at a large angle, and a larger angle error is generated compared with the calibrated result. For the calibration of such samples, a mode of moving the sample stage is usually adopted, and the calibration speed is limited by the mechanical movement of the sample stage, and is extremely slow, about 10 seconds per point.
Therefore, EBSD has long been recognized as a means of characterizing "microtexture" (i.e., microrelief texture).
In recent years, the characterization speed of EBSD has been greatly increased under the efforts of EBSD equipment manufacturers. At present, the speed of the fastest EBSD probe reaches 3000 points/second, but the speed is achieved under an ideal condition, namely, the speed can be achieved when a coarse grain deformation-free sample is calibrated by using an ultra-large electron beam, in an actual test, the calibration speed generally does not exceed 100 points/second, and a better solution scheme still does not exist for the calibration of the coarse grain sample.
Therefore, the invention aims to combine a series of morphology characterization technologies with a computer graphic identification technology under the conditions of the existing scanning electron microscope and EBSD system, assist the EBSD system to accurately determine the EBSD scanning coordinate, quickly obtain large-area crystallographic orientation information of the crystalline material and calculate the accurate macro texture of the material.
Disclosure of Invention
The invention aims to solve the technical problem of improving the EBSD characterization crystal material texture efficiency and accuracy.
The technical scheme for solving the technical problems is as follows: a method for EBSD rapid characterization of texture comprises the following steps:
s1: obtaining a sample and obtaining the overall size of the sample;
s2: obtaining a crystal grain topography of the sample;
s3: digitizing the crystal grain topography and recording the position coordinates of the central point of each crystal grain;
s4: calibrating the center point of each crystal grain to obtain the crystal orientation of the center of each crystal grain;
s5: generating EBSD data of the calibrated area;
s6: and obtaining texture information of the sample according to the EBSD data of the calibration area.
The beneficial effects of the invention are: (ii) a Within a grain, the orientation difference between each part is usually very small, even if there is a defect such as dislocation, different parts have certain orientation difference, the orientation difference is much less than 2 °, which is generally considered as reliable angular resolution of EBSD, if within a grain, a sub-crystal structure is formed due to deformation, and the like, the sub-crystal structure can be distinguished by ECC technology, and is displayed as a sub-crystal grain on an ECC image, which is directly identified as a grain in the technology, but for coarse grains on a large-size sample, the coarse grains are large-angle grain boundaries, and are easy to corrode and identify, therefore, the orientation of the center of the grain is mainly used to represent the orientation of the whole grain, compared with the general method for calibrating texture, the method can improve the speed of EBSD testing texture by 30-100 times, and is more obvious in calibration of mixed crystal sample, and at the same time, the method has the advantages that the characterization of the crystal boundary is more accurate, no matter the grain boundary is an ECC image, or an image is formed by a digital camera or a scanner, the pixel density can be very high, and the reproducibility of the crystal boundary is far superior to that of the crystal boundary reconstructed by traditional EBSD data with only 5-10 pixels in each direction, so that the technical problem of how to improve the EBSD characterization efficiency and accuracy of the crystal material texture is solved.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, step S1 specifically includes: obtaining a sample and obtaining the overall size of the sample;
step S2 specifically includes:
step S21: when the overall dimension is 10 x 10mm2If so, executing step S22, otherwise, executing step S23;
step S22: obtaining an ECC image of the sample through a backscattering probe, taking the ECC image as a grain topography, and executing step S3;
step S23: and pretreating the sample, slightly corroding the surface of the sample, recording a profile diagram of the grain boundary, and taking the profile diagram as a grain morphology diagram.
The benefit of using the above further scheme is that such ECC is like a grain topography on the sample, since the electron channel contrast is particularly sensitive to the crystallographic orientation of the material.
Further, in step S23, the sample may be pretreated by mechanically polishing and electropolishing the sample.
The method has the advantages that the sample with a smooth surface can be obtained, and the residual stress on the surface of the sample can be removed.
Further, in step S4, the electron beam is moved to the center point of each of the crystal grains of the sample, the back scattering diffraction pattern is calibrated, the crystal orientation of each of the crystal grain centers is obtained, and the euler angle is recorded.
Further, step S5 is specifically to determine the crystal orientation as the overall orientation of the crystal grain, mark the orientations corresponding to all coordinate points in the crystal grain as the orientation, and synthesize the coordinates and orientation data of all crystal grains into EBSD data of the marked region.
Advantages of additional aspects of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a flowchart of a method of an embodiment of the EBSD method for rapid texture characterization of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
The embodiment is basically as shown in the attached figure 1:
the method for rapidly characterizing the texture by the EBSD in this embodiment includes the following steps: s1: obtaining a sample, and obtaining the overall size of the sample;
s2: obtaining a crystal grain topography of a sample;
s3: digitizing the crystal grain topography and recording the position coordinates of the central point of each crystal grain;
s4: calibrating the center point of each crystal grain to obtain the crystal orientation of the center of each crystal grain;
s5: generating EBSD data of the calibrated area;
s6: and obtaining the texture information of the sample according to the EBSD data of the calibration area.
The invention has the beneficial effects that: (ii) a Within a grain, the orientation difference between each part is usually very small, even if there is a defect such as dislocation, different parts have certain orientation difference, the orientation difference is much less than 2 °, which is generally considered as reliable angular resolution of EBSD, if within a grain, a sub-crystal structure is formed due to deformation, and the like, the sub-crystal structure can be distinguished by ECC technology, and is displayed as a sub-crystal grain on an ECC image, which is directly identified as a grain in the technology, but for coarse grains on a large-size sample, the coarse grains are large-angle grain boundaries, and are easy to corrode and identify, therefore, the orientation of the center of the grain is mainly used to represent the orientation of the whole grain, compared with the general method for calibrating texture, the method can improve the speed of EBSD testing texture by 30-100 times, and is more obvious in calibration of mixed crystal sample, and at the same time, the method has the advantages that the characterization of the crystal boundary is more accurate, no matter the grain boundary is an ECC image, or an image is formed by a digital camera or a scanner, the pixel density can be very high, and the reproducibility of the crystal boundary is far superior to that of the crystal boundary reconstructed by traditional EBSD data with only 5-10 pixels in each direction, so that the technical problem of how to improve the EBSD characterization efficiency and accuracy of the crystal material texture is solved.
On the basis of the technical scheme, the invention can be further improved as follows.
Optionally, in some other embodiments, step S1 specifically includes: obtaining a sample, and obtaining the overall size of the sample;
step S2 specifically includes:
step S21: when the overall size is 10 multiplied by 10mm2If so, executing step S22, otherwise, executing step S23;
step S22: obtaining an ECC image of the sample through a backscattering probe, taking the ECC image as a grain topography, and executing the step S3;
step S23: and (3) pretreating the sample, slightly corroding the surface of the sample, recording a profile diagram of a grain boundary, and taking the profile diagram as a grain morphology diagram.
Such an ECC is like a grain topography on a sample, since the electron channel contrast is particularly sensitive to the crystallographic orientation of the material.
Alternatively, in some other embodiments, the pretreatment of the sample in step S23 may be mechanical polishing and electropolishing.
A sample with a smooth surface can be obtained, and the residual stress on the surface of the sample is removed.
Alternatively, in some other embodiments, step S4 is embodied by moving the electron beam to the center of each grain of the sample, calibrating the backscatter diffraction pattern, obtaining the crystal orientation of each grain center, and recording the euler angle.
Optionally, in some other embodiments, step S5 specifically includes determining a crystal orientation as the overall orientation of the crystal grain, marking orientations corresponding to all coordinate points in the crystal grain as the orientation, and synthesizing coordinates and orientation data of all crystal grains into EBSD data of the marked region.
It should be noted that the above embodiments are product embodiments corresponding to the above method embodiments, and for the description of each structural device and the optional implementation in this embodiment, reference may be made to the corresponding description in the above method embodiments, and details are not repeated here.
The reader should understand that in the description of this specification, reference to the description of the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
It is clear to those skilled in the art that, for convenience and brevity of description, the specific working processes of the above-described apparatuses and units may refer to the corresponding processes in the foregoing method embodiments, and are not described herein again.
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. A method for EBSD rapid characterization of texture is characterized by comprising the following steps:
s1: obtaining a sample and obtaining the overall size of the sample;
s2: obtaining a crystal grain topography of the sample;
s3: digitizing the crystal grain topography and recording the position coordinates of the central point of each crystal grain;
s4: calibrating the center point of each crystal grain to obtain the crystal orientation of the center of each crystal grain;
s5: generating EBSD data of the calibrated area;
s6: obtaining texture information of the sample according to the EBSD data of the calibration area;
step S1 specifically includes: obtaining a sample and obtaining the overall size of the sample;
step S2 specifically includes:
step S21: when the overall dimension is 10 x 10mm2If so, executing step S22, otherwise, executing step S23;
step S22: obtaining an ECC image of the sample through a backscattering probe, taking the ECC image as a grain topography, and executing the step S3;
step S23: and pretreating the sample, slightly corroding the surface of the sample, recording a profile diagram of a grain boundary, and taking the profile diagram as a grain morphology diagram.
2. The method for EBSD fast characterization of texture according to claim 1, characterized by: in step S23, the sample is pre-treated, specifically by mechanically polishing and electropolishing the sample.
3. The method for EBSD fast characterization of texture according to claim 1, characterized by: step S4 is to move the electron beam to the center of each grain of the sample, calibrate the back scattering diffraction pattern, obtain the crystal orientation of each grain center, and record the euler angle.
4. The method for EBSD fast characterization of texture according to claim 1, characterized by: step S5 is specifically to determine the crystal orientation as the overall orientation of the crystal grain, mark the orientations corresponding to all coordinate points in the crystal grain as the orientation, and synthesize the coordinates and orientation data of all crystal grains into EBSD data of a marked region.
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| CN111289546B (en) * | 2020-04-02 | 2021-04-13 | 贵研检测科技（云南）有限公司 | Preparation and characterization method of precious metal superfine wire EBSD test sample |
| CN114047211B (en) * | 2021-11-10 | 2023-03-28 | 北京理工大学 | Method for detecting austenite grain diameter of elastic steel material based on EBSD |
| CN115662553B (en) * | 2022-12-13 | 2023-03-21 | 北京科技大学 | Method for constructing material microstructure information database |
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